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Rheological Characterization
Annika Björn, Paula Segura de La Monja,
Anna Karlsson, Jörgen Ejlertsson and Bo H. Svensson
Department of Thematic Studies, Water and Environmental Studies,
Linköping University,
Sweden
1. Introduction
The biogas process has long been a part of our biotechnical solutions for the handling of
sewage sludge and waste. However, in many cases the existing process applications need to
be optimized to improve the extent of biogas production as a part of the energy supply in a
sustainable and viable society. Although the principles are well known, process
disturbances and poor substrate utilization in existing biogas plants are common and are in
many cases likely linked to changes in the substrate composition.
Changes in substrate composition can be done as a means to obtain a more efficient
utilization of existing biogas facilities, which today treating mainly manure or sewage
sludge. By bring in more energy rich residues and wastes a co-digestion process with higher
biogas potential per m3 volatile solids (VS) can often be obtained. However, new and
changing feedstocks may result in shift in viscosity of the process liquid and, hence,
problems with inadequate mixing, break down of stirrers and foaming. These disturbances
may seriously affect the degradation efficiency and, hence, also the gas-production per unit
organic material digested. In turn, operational malfunctions will cause significant logistic
problems and increased operational costs. Changes of the substrate profile for a biogas plant
may also infer modifications of the downstream treatment of the digestate.
Together with high digestion efficiency, i.e. maximum methane formation per reactor
volume and time, the economy of a biogas plant operation depends on the energy invested
to run the process. A main part of the energy consumed during operation of continuous
stirred tank reactors (CSTRs) is due to the mixing of the reactor material (Nordberg and
Edström, 2005). The shear force needed is dependent on the viscosity of the reactor liquid,
where increasing viscosity demands a higher energy input. Active stirring must be
implemented in order to bring the microorganisms in contact with the new feedstock, to
facilitate the upflow of gas bubbles and to maintain an even temperature distribution in the
digester. Up to 90% of biogas CSTR plants use mechanical stirring equipment (Weiland et
al., 2010).
In this context the rheological status of the reactor liquid as well as of the residual digestate
are important for process mixing design and dimensioning. In addition experiences on
rhelogical characterisation of sewage sludge revealing their dependence on the suspended
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64 Biogas
solid concentration and on the characteristics of the organic material as well as on the
interactions between particles and molecules in the solution (Foster, 2002). Therefore, this
type of characterisation can be important in process monitoring and control.
The aim of this chapter is to briefly introduce the area of rheology and to present important
parameters for rheological characterization of biogas reactor fluids. Examples are given
from investigations on such parameters for lab-scale reactors digesting different substrates.
2. Rheology
Rheology describes the deformation of a body under the influence of stress. The nature of
the deformation depends on the body’s material conditions (Goodwin & Hughes, 2000).
Ideal solids deform elastically, which means that the solid will deform and then return to its
previous state once the force ceases. In this case, the energy needed for deformation will
mainly be recovered after the stress terminates. If the same force is applied to ideal fluids, it
will make them flow and the energy utilized will disperse within the fluid as heat. Thus, the
energy will not be recovered once the forcing stress is terminated (Goodwin & Hughes,
2000).
For fluids a flow curve or rheogram is used to describe rheological properties. These
properties may be of importance in anaerobic digestion for the dimensioning of e.g. feeding,
pumping and stirring. Rheograms are constructed by plotting shear stress (τ) as a function
of the shear rate () (Tixier et al., 2003; Guibad et al., 2005).
The stress applied to a body is defined as the force (F) divided by the area (A) over which
this force is acting (Eq. 1). When forces are applied in opposite directions and parallel to the
side of the body it is called shear stress (Goodwin & Hughes, 2000). Shear stress (τ; Pa) is
one of the main parameters studied in rheology, since it is the force per unit area that a fluid
requires to start flowing (Schramm, 2000). The shear rate (; s-1) describes the velocity
gradient (Eq. 2). Hence, shear rate is the speed of a fluid inside the parallel plates generated
when shear stress is applied (Pevere & Guibad, 2005).
equation (Eq. 3) illustrates the flow behaviour of an ideal liquid (Schramm, 2000), where is
illustrated for glycerol in figure 1, and are identified as Newtonian fluids. The Newtonian
the viscosity (Pa*s). Dynamic viscosity, also called apparent viscosity, describes a fluid’s
resistance of deformation (Pevere & Guibad, 2005). In terms of rheology it is the relation of
τ=* (3)
=/ (4)
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Rheological Characterization 65
When measuring the dynamic viscosity, the fluid is subjected to a force impact caused by
moving a body in the fluid. Resistance to this movement provides a measure of fluid
viscosity. The dynamic viscosity can be measured using a rotation rheometer. The device
consists of an external fixed cylinder with known radius and an internal cylinder or spindle
with known radius and height. The space between the two cylinders is filled with the fluid
subjected to dynamic viscosity analysis.
130
Pa
110
100
90
80
70
60
50
40
30
20
10
0
0 100 200 300 400 500 600 700 1/s 800
Shear Rate
.
Fig. 1. Rheogram – flow curve of glycerol (▲) at 20 °C with a linear relationship between
shear stress (; Pa) and shear rate (; s-1), representing a Newtonian liquid.
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66 Biogas
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Rheological Characterization 67
start flowing. One type of these, the Bingham plastic, requires the shear stress to exceed a
minimum yield stress value in order to go from high viscosity to low viscosity. After this
change a linear relationship between the shear stress and the shear rate will prevail (Ryan,
2003). Examples of Bingham plastic liquids are blood and some sewage sludge’s.
τ = 0 + * n (5)
be able to compare -values for different fluids they should have similar flow behaviour
The consistency index parameter () gives an idea of the viscosity of the fluid. However, to
index (n). When the flow behaviour index is close to 1 the fluid´s behaviour tends to pass
from a shear thinning to a shear thickening fluid. When n is above 1, the fluid acts as a shear
thickening fluid. According to Seyssiecq and Ferasse (2003) equation 5 gives fluid behaviour
information as follows:
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68 Biogas
τ = * (n-1) (6)
n < 1 Pseudoplastic behaviour
n = 1 Newtonian behaviour
n > 1 Dilatant behaviour
= 0 + * (7)
0 = 0 Newtonian behaviour
0 > 1 Bingham plastic behaviour
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Rheological Characterization 69
Rheological measurements were carried out with a three-step protocol where (1) the shear
rate increased linearly from 0 to 800 s-1 in 800 sec., (2) maintaining constant shear rate at 800
s-1 in 30 sec, (3) decreasing linearly the shear rate from 800 to 0 s-1 in 800 sec., according to
Björn et al. (2010). For each sample three measurements were carried out and performed
immediately after sampling or stored at +4 ºC pending analysis.
The fluid behaviour was interpreted by the flow- and viscosity curves according to
Schramm (2000), and the dynamic viscosity, limit viscosity and yield stress were noticed.
The three most common mathematical models for non-Newtonian fluids; Herschel Bulkley
model; Ostwald model (Power Law) and Bingham model, were applied in order to
transform rheogram data values to the rheological behaviour of the fluids. Flow behaviour
index (n) and consistency index (K) were studied.
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70 Biogas
between the curves was noticeable when the shear rate increased and afterwards decreased
for reactor B (Fig. 2). This area describes the degree of thixotropy of this fluid, which means
that the increase of this area is related to the amount of energy required to breaking down
the thixotropic structure. Thus, the flow curves obtained with the three-step protocol
indicated a thixotropic behaviour of reactor fluid B.
30
Pa
26
24
22
20
18
16
14
12
10
8
6
4
2
0
0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 1/s 800
Shear Rate
.
Fig. 2. Rheogram - flow curves illustrating shear stress (; Pa) vs shear rate (; s-1) for fluids
from reactor A (▲), B (▲) and C (▲) with a three-step protocol.
Reactors C and E revealed viscoplastic behaviours, i.e. a pseudoplastic behaviour with yield
stress. Reactor C, fed with biosludge from paper mill industry 2, showed a yield stress of 4
Pa (Fig. 2), and reactor E, receiving cereal residues, a yield point of 4.5 Pa (Fig. 3). The yield
stress is defined as the force that a fluid must overcome in order to start flowing (Spinosa &
Lotito, 2003). Also for reactor E, a small space between the curves was noticeable when the
shear rate increased and afterwards decreased (Fig. 3). This area difference might indicate
some degree of thixotropy.
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Rheological Characterization 71
5
30 10
Pa Pa·s
4
26 10
24
3
22 10
20
2
18 10
16
1
10
14
12 0
10
10
8 -1
10
6
4 -2
10
2
-3
0 10
0 100 200 300 400 500 600 700 1/s 800
Shear Rate
.
Fig. 3. Rheogram - flow and viscosity curves for reactors D (▲; ●) and E (▲; ●) with a three-
step protocol. Flow curves illustrating shear stress (; Pa) vs shear rate (; s-1) and viscosity
curves illustrating dynamic viscosity (; Pa*s) vs shear stress (; s-1).
30 1 000 000
Pa Pa·s
100 000
26
24
10 000
22
20 1 000
18
100
16
14
10
12
10 1
8
0,1
6
4
0,01
2
0 0,001
0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 1/s 800
Shear Rate
.
Fig. 4. Rheogram - flow and viscosity curves for reactors A (▲;●), B (▲;●) and C (▲;●) with
a three-step protocol. Flow curves illustrating shear stress (; Pa) vs shear rate (; s-1) and
viscosity curves illustrating dynamic viscosity (; Pa*s) vs shear stress (; s-1).
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72 Biogas
The viscosity curves (Figures 3−4) did almost correspond to the flow curve behaviour for
the investigated biogas reactor fluids (Table 2). Using the scheme by Schramm (2000) the
viscosity curves for reactor A indicated a viscoplastic liquid and for reactor D a viscoplastic
or pseudoplastic liquid. The viscosity initially dropped very quickly for reactor A,
specifically indicating Bingham viscoplastic fluids with pseudo-Newtonian behaviour.
Generally for reactors A−E, the viscosity decreased with increasing shear rate, until it
reached its limit viscosities (Table 3).
Table 3. The initial dynamic viscosity and the limit viscosity obtained during interval 1 in
the 3-step protocol analysis for each reactor fluid.
The limit viscosities ranged 6−36 mPa*s with the highest value for reactor E (Table 3).
However, the limit viscosity was similar for reactor C and E despite a difference in TS (%).
The dynamic viscosity ranged 18−443 mPa*s for the reactor fluids (Table 3). The reactors A
and D showed lower dynamic viscosity values compared to reactor B, C and E, possibly due
to their pseudo-Newtonian behaviour. Also, there was a difference in dynamic viscosity
between reactor fluids B and C both receiving biosludge with similar TS (%) but coming
from two different paper mill industries in Sweden. Thus, the results demonstrated that
similar TS values do not necessarily correspond to similar dynamic or limit viscosity values.
This contradicts the results presented by Tixier and Guibad (2003), who reported that an
increase in TS for activated sludge corresponded to a higher limit viscosity and higher yield
stress. Nor, did biosludge from two different Swedish pulp- and paper mill industries with
similar TS give similar viscosity values.
Samples from reactor B showed different rheological behaviour depending on when they
were measured. The yield stress and viscosity increased when the reactor fluids had been
stored and resting compared to when analyzed immediately after sampling, indicating
thixotropic behaviour. Figure 5 illustrates how the B reactor fluid after been resting for 48
hours showed a resistance to flow, known as static yield stress. This value (24 Pa) decreased
until it reached the dynamic yield stress (7 Pa), which was the value needed in order to
become liquid and start flowing. When the analysis was done right after the first
measurement (Second measurement), the fluid had already been stirred, so the two different
structures that form the resistance to flow were now mixed and no static yield stress was
detected. The static yield stress might be initiated by several factors, e.g. weakness of the
fluid structure, low mixed liquid solid suspension (MLSS) concentration, small size of
particles and poor dewater ability (Pevere et al. 2006).
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Rheological Characterization 73
Fig. 5. Rheogram – shear stress (; Pa) vs shear rate (; s-1) of reactor B. Four measurements
of the same sample were made after different sample resting times (1st▲; 2nd▲; 3rd▲;
4th ▲).
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74 Biogas
corresponded to a low consistency value (5*10-10). At the static yield stress of 24 Pa (Fig. 5),
the flow behaviour index showed shear thickening fluid behaviour (n=1.41) and a limit
viscosity of 22 mPa*s. This also corresponded to a low consistency value (5*10-4). As soon as
the fluid was measured again, n decreased (0.70) showing a pseduoplastic behaviour and K
increased (0.11) indicating that the consistency of the reactor material was higher. The limit
viscosity was 17 mPa*s. These results showing a time dependency and structure recovery
strengthen the arguments for a thixotropic fluid behaviour of reactor B. Once the stirring has
ended and the fluid was at rest, the fluid structure starts to rebuild. Therefore, the viscosity
become time dependent. This information is important to consider for biogas reactor
performance, e.g. when applying semi-continuous mixing.
0 n R2 n R2 0 R2
reactors A−E. 0: yield stress (Pa); n: flow behaviour index; : Consistency index; R2:
Table 4. The results obtained from mathematical modelling of rheogram data of fluids from
regression coefficient.
Also, fluids from reactor C and E were hard to define from modelling of the rheogram data
because they gave indications for fluids being between pseudoplastic and Bingham plastic
behaviours, i.e. the 0-values were >0 (2.89 and 2.38) and n <1 (Table 4).
4. Conclusion
The biogas reactor fluids investigated were behaving viscoplasticly, since they had yield
stress and one of them was also thixotropic, due to its partial structure recovering. However,
the reactor treating slaughterhouse waste was very close to act as a Newtonian fluid. Also,
there was a difference in dynamic- and limit viscosities depending on the substrates used.
The results demonstrated that similar TS values did not necessarily correspond to similar
flow and viscosity behaviours. Nor, did biosludge from two different Swedish paper mill
industries with similar TS show similar viscosity values.
To encounter problems related to involvement of new substrates and/or co-digestions in
existing facilities, investigations for possible viscosity changes are needed. Ongoing research
will hopefully provide an important basis for predictions of changes in rheology linked to
the composition of the organic materials, which are translated in the process. This is
important in order to achieve proper designs in relation to possible variation in substrate
mixes in conjunction with new constructions, but also to better control material flows in the
existing facilities to avoid disturbances in the reactor performance.
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Rheological Characterization 75
5. References
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suspensions: application to pasty sewage sludges. Jour Rheol, Vol.45, No.5, pp.
1123-1139.
Björn, A. ; Segura de La Monja, P. ; Karlsson, A. ; Ejlertsson, J. & Svensson, BH. (2010).
Differences and shifts in the rheological characteristics of fluids in controlled
stirred tank reactors for biogas production. Poster presentation at World
Conference in Anaerobic Digestion (AD12), Guadalajara, Mexico October 31rd o
November 4th 2010.
Foster, CF. (2002). The rheological and physico-chemical characteristics of sewage sludges.
Enzyme Microb Technol, Vol.30, pp. 340-345.
Goodwin, JW. & Hughes, RW. (2000). Rheology for Chemists, an introduction. Royal Society of
Chemist. Cambridge, UK.
Guibad, G.; Tixier, N. & Baudu, M. (2005). Hysteresis area, a rheological parameter used as a
tool to assess the ability of filamentous sludges to settle. Process Biochem, Vol.40, pp.
2671-2676.
Lotito, V.; Spinosa, L.; Minini, G. & Antonaci, R. (1997). The rheology of sewage sludge at
different steps of treatment. Water Sci Tech, Vol.36, No.11, pp. 79-85.
Menéndez, M. & Paredes, B. (2006). Rheological behaviour and organoleptic effects of
ovalbumin addition in yoghurt mousse production. Jour Dairy Sci, Vol.89, pp.
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Morgavi, DP.; Beauchemin, KA. & Nsereko, LM. (2001). Resistance of feed enzymes to
proteolytic inactivation by rumen microorganisms and gastrointestinal proteases.
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Nordberg, Å. & Edström, M. (2005). Co-digestion of energy crops and the source-sorted
organic fraction of municipal solid waste. Water Sci Tech, Vol.52, No.1-2, pp.
217-222.
Pevere, A. & Guibad, G. (2005). Viscosity evolution of anaerobic granular sludge. Biochem
Engin Jour, pp. 315-322.
Pevere, Å.; Guibad, G; van Hullenbusch, E.; Lens, P. & Baudu, M. (2006). Viscosity evolution
of anaerobic granular sludgee. Biochem Engin Jour, Vol.27, pp. 315.322
Schramm, G. (2000). A practical Approach to Rheology and Rheometry, (2nd Ed.), Thermo Haake
Rheology, Germany
Seyssiecq, I.; Ferasse, J.H. & Roche, N. (2003). State-of-the-art: rheological characterization of
waste water treatment sludge. Biochem Engin Jour, Vol.16, pp. 41-56.
Spinosa, L., & Lotito, V. (2003). A simple method for evaluating yield stress. Adv Environ
Research, Vol.7, pp. 655-659.
Tixier, N.; Guibad, G. & Baudu, M. (2003). Determination of some rheological
parameters for the characterization of activated sludge. Bioresource Tech, Vol.90,
pp. 215-220.
Weiland, P. (2010). Biogas production: current state and perspectives. Appl Microbiol
Biotechnol, Vol.85, pp. 849-860.
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76 Biogas
Yang, F. ; Bick, A. & Shandalov, S. (2009). Yield stress and rheological characteristics of
activated sludge in an airlift membrane bioreactor. Jour Membrane Sci, Vol.334, pp.
83-90.
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Biogas
Edited by Dr. Sunil Kumar
ISBN 978-953-51-0204-5
Hard cover, 408 pages
Publisher InTech
Published online 14, March, 2012
Published in print edition March, 2012
This book contains research on the chemistry of each step of biogas generation, along with engineering
principles and practices, feasibility of biogas production in processing technologies, especially anaerobic
digestion of waste and gas production system, its modeling, kinetics along with other associated aspects,
utilization and purification of biogas, economy and energy issues, pipe design for biogas energy,
microbiological aspects, phyto-fermentation, biogas plant constructions, assessment of ecological potential,
biogas generation from sludge, rheological characterization, etc.
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Annika Björn, Paula Segura de La Monja, Anna Karlsson, Jörgen Ejlertsson and Bo H. Svensson (2012).
Rheological Characterization, Biogas, Dr. Sunil Kumar (Ed.), ISBN: 978-953-51-0204-5, InTech, Available
from: http://www.intechopen.com/books/biogas/rheological-characterization